CN102030555B - Method for preparing thick carbon/carbon heat insulation cover for polysilicon hydrogenation furnace - Google Patents
Method for preparing thick carbon/carbon heat insulation cover for polysilicon hydrogenation furnace Download PDFInfo
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Abstract
The invention discloses a method for preparing a thick carbon/carbon heat insulation cover for a polysilicon hydrogenation furnace, comprising the following steps: 1. adopting carbon cloth and short carbon fibers to prepare a quasi-three-dimensional preform; 2. mixing epoxy resins, a diluting agent and a curing agent to prepare epoxy resin glue solution; 3. spraying or brushing the epoxy resin glue solution on the surface of the quasi-three-dimensional preform to form a coating and then curing the quasi-three-dimensional preform to harden and shape the surface of the quasi-three-dimensional preform; 4. impregnating the cured quasi-three-dimensional preform into an impregnating tank; 5. carbonizing the impregnated quasi-three-dimensional preform; and 6. carrying out chemical vapor deposition (CVD) coating processing on the preform after mechanical processing to obtain the carbon/carbon heat insulation cover for the polysilicon hydrogenation furnace. The method has the following advantages: the molding process is simple, the manufacturing cost is lower, and the prepared carbon/carbon heat insulation cover has the characteristics of good heat insulation effect, excellent gas erosion resistance and good mechanical property.
Description
Technical field
The invention belongs to carbon/carbon insulating material technology field, be specifically related to a kind of preparation method of thick carbon/carbon heat insulation cover for polysilicon hydrogenation furnace.
Background technology
At present, the main method of producing polysilicon is improved Siemens, adopts the polysilicon of improved Siemens production to account for more than 80% of global polysilicon ultimate production.When improved Siemens was produced polysilicon product, hydrogenation furnace was that the recycle system is the step that reaction product reclaims, and was about to generate the by product SiCl that the reaction of polysilicon goods produces
4With H
2Reaction generates SiHCl
3Raw material re-uses.Hydrogenation furnace thermal field product comprises stay-warm case, thermoscreen, heating element and heat insulation bottom board, wherein, stay-warm case is positioned at the outer furnace shell of thermoscreen, plays the effect of heat preservation energy-saving, guarantee that namely thermoscreen inside reaches hydrogenation furnace and reacts desired temperature, and the stay-warm case outside temperature is lower.Polysilicon hydrogenation furnace is used stay-warm case by graphite or is solidified the insulation quilt manufacturing at present, because graphite product intensity is low, thermal conductivity is high, and the high temperature heat-resistant shock stability is poor, and work-ing life is short, change frequent, the large size goods difficulty that is shaped makes its requirement that is difficult to satisfy the production of polysilicon development, and solidifies insulation quilt because its density is lower and work out by staple fibre, thereby erosion resistibility is low in use, easily fall the work-ing life that slag reduces goods, increases the number of times of its replacing.
Grant number is to disclose the charing of a kind of employing acetone-furfural resin dipping in the patent of CN101063223, mechanical workout makes the preparation method that monocrystalline silicon draw machines is used carbon/carbon thermal insulation cover after the purification process, grant number is that the patent of CN101269981 has been announced a kind of employing acetone-furfural resin or the charing of ammonia resin impregnating, mechanical workout makes the preparation method of high temperature furnace used carbon/carbon heat insulation bottom board after the purification process, its weak point is: (1) the method is directly carried out the resin vacuum impregnation charing with precast body and is processed, cause heat-preservation cylinder cylinder section product to occur oval, the heat-preservation cylinder flat cover, the problem on deformation such as warpage appear in heat insulation bottom board; (2) stay-warm case, the heat insulation bottom board the finished product surface of the method preparation are unprocessed, but machine namely obtains product after adding, and cause product slag, decortication in use to occur falling and pollute product in the stove.
Grant number is that the patent of CN101445377 discloses a kind of employing CVI and processes and carry out the resin vacuum impregnation charing after will the goods typing and process, then paste the graphite paper charing and make the preparation method of high temperature furnace used carbon/carbon insulating cylinders, the weak point of the method is (1) employing chemical vapour deposition typing precast body, cost is higher, complex technical process, and adopt chemical vapour deposition density effect relatively poor for thick size product, do not have the effect of typing; (2) graphite paper easily comes off in High Temperature Furnaces Heating Apparatus, thereby pollutes product in the stove.
Summary of the invention
Technical problem to be solved by this invention is for above-mentioned the deficiencies in the prior art, provides a kind of moulding process simple, the preparation method of the thick carbon/carbon heat insulation cover for polysilicon hydrogenation furnace that manufacturing cost is lower.The polysilicon hydrogenation furnace of preparation is good with high insulating effect, anti-air scour excellent performance, the mechanical property of carbon/carbon thermal insulation cover.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of preparation method of thick carbon/carbon heat insulation cover for polysilicon hydrogenation furnace, it is characterized in that, and the method may further comprise the steps:
(1) adopt charcoal cloth and short carbon fiber to prepare pseudo-three-dimensional preform; The density of described pseudo-three-dimensional preform is 0.20g/cm
3～0.50g/cm
3, thickness is 100mm～220mm;
(2) at normal temperatures Resins, epoxy, thinner and solidifying agent are mixed and made into epoxy resin adhesive liquid by 100: 5～10: 8～20 mass ratio; Described thinner is alcohol, acetone, toluene or epoxide resin reactive diluent, and described solidifying agent is diethylenetriamine, quadrol, triethylene tetramine or polymeric amide;
(3) with epoxy resin adhesive liquid described in the step (2) spraying or brush that to form thickness in the surface of pseudo-three-dimensional preform described in the step (1) be the coating of 0.5mm～5mm, then will form pseudo-three-dimensional preform after the coating and solidify the pseudo-three-dimensional preform surface hardening is finalized the design;
(4) pseudo-three-dimensional preform after solidifying in the step (3) is placed impregnating autoclave, adopt ammonia resol as soaker, flood 4h～12h vacuumizing under the condition; The viscosity of described ammonia resol is 150mPas～500mPas, and the solids content of described ammonia resol is 40%～60%;
(5) pseudo-three-dimensional preform behind dipping in the step (4) is placed charring furnace, under the condition that vacuumizes, carry out charing and process, when the density of pseudo-three-dimensional preform reaches 0.60g/cm
3～0.90g/cm
3In time, stops charing and processes, and furnace cooling obtains precast body;
(6) precast body described in the step (5) is carried out mechanical workout, then the precast body after the mechanical workout being placed chemical vapor deposition stove to carry out the CVD coating processes, stopping the CVD coating after the precast body surface forms the coating that thickness is 5 μ m～150 μ m processes, it is 1000mm～1800mm that furnace cooling namely obtains diameter, highly be 200mm～1500mm, thickness is the polysilicon hydrogenation furnace carbon/carbon thermal insulation cover of 80mm～220mm.
Epoxide resin reactive diluent described in the above-mentioned steps (2) is butylglycidyl ether, epoxy propane butyl ether, propylene oxide phenyl ether or ethylene glycol diglycidylether.
The system of solidifying described in the above-mentioned steps (3) is: place at normal temperatures 48h above solidify or place in the curing oven under temperature is 40 ℃～80 ℃ condition solidify 2h～8h.
The temperature that charing described in the above-mentioned steps (5) is processed is 900 ℃～1200 ℃.
The system that CVD coating described in the above-mentioned steps (6) is processed is: adopting propylene or Sweet natural gas as presoma, is to carry out the CVD coating under 800 ℃～1100 ℃ the condition to process in temperature.
The present invention compared with prior art has the following advantages:
1, the structure of pseudo-three-dimensional preform prevented goods make and use procedure in layering or cracking, compare early stage stay-warm case of precast body thickness has increased by 2～4 times, has greatly improved the heat preservation and energy conservation effects of goods.
2, adopt the Resins, epoxy brush coating with the precast body solidifying and setting, technological process is simple, and fixed effect is remarkable, prevents that distortion from appearring in product in subsequent technique, reduces cost, reduces the production cycle.
3, carrying out charing behind the employing ammonia resin impregnating under vacuum state processes, reduced the foreign matter content of goods, compactness extent is suitable, can effectively reduce polysilicon hydrogenation furnace good with thermal conductivity, the process consistency of carbon/carbon thermal insulation cover, exploitativeness is strong, and cost is low.
4, adopt CVD top coat treatment technology, improve product surface smooth finish, improve the erosion resistibility of goods, and so that the mechanical property of goods is improved, prolonged work-ing life.
5, this Technology moulding process is simple, and manufacturing cost is lower, and the polysilicon hydrogenation furnace that makes is good with carbon/carbon thermal insulation cover high insulating effect, anti-air scour excellent performance, mechanical property.
Embodiment
Embodiment 1
(1) adopt charcoal cloth and short carbon fiber net tire alternative stacked, consist of the in-plane fiber, adopt needling process to introduce vertical fibers at thickness direction, making density is 0.20g/cm
3, thickness is the pseudo-three-dimensional preform of 100mm;
(2) at normal temperatures Resins, epoxy, thinner and solidifying agent are mixed and made into epoxy resin adhesive liquid by 100: 5: 8 mass ratio; Described thinner is alcohol, and described solidifying agent is diethylenetriamine;
(3) epoxy resin adhesive liquid is brushed to form thickness in pseudo-three-dimensional preform surface be the coating of 0.5mm, then will form pseudo-three-dimensional preform after the coating and place at normal temperatures that 48h is above to be solidified, the pseudo-three-dimensional preform surface hardening is finalized the design;
(4) pseudo-three-dimensional preform after solidifying is placed impregnating autoclave, adopting viscosity is 150mPas, solids content be 40% ammonia resol as soaker, flood 4h vacuumizing under the condition;
(5) pseudo-three-dimensional preform behind dipping being placed charring furnace, is to carry out charing under 900 ℃ the vacuum condition to process in temperature, when the density of pseudo-three-dimensional preform reaches 0.60g/cm
3In time, stops charing and processes, and furnace cooling obtains precast body;
(6) precast body is carried out mechanical workout, then the precast body after the mechanical workout is placed chemical vapor deposition stove, adopt propylene as presoma, be to carry out the CVD coating under 800 ℃ the condition to process in temperature, forming thickness on the precast body surface is the coating of 5 μ m, it is 1000mm that furnace cooling namely obtains diameter, highly is 200mm, and thickness is the polysilicon hydrogenation furnace carbon/carbon thermal insulation cover of 80mm.
The polysilicon hydrogenation furnace of the present embodiment preparation is 20MPa with the tensile strength of carbon/carbon thermal insulation cover, and compressive strength is 40MPa, and flexural strength is 35MPa, and thermal conductivity is 1W/mk (800 ℃).
Embodiment 2
The present embodiment is identical with embodiment 1 preparation method, wherein difference is: described thinner is acetone, toluene, butylglycidyl ether, epoxy propane butyl ether, propylene oxide phenyl ether or ethylene glycol diglycidylether, described solidifying agent is quadrol, triethylene tetramine or polymeric amide, adopts Sweet natural gas as presoma.
The polysilicon hydrogenation furnace of the present embodiment preparation is 15MPa～25MPa with the tensile strength of carbon/carbon thermal insulation cover, compressive strength is 30MPa～50MPa, flexural strength is 25MPa～40MPa, and thermal conductivity is 0.3W/mk (800 ℃)～1.5W/mk (800 ℃).
Embodiment 3
(1) adopt charcoal cloth and short carbon fiber net tire alternative stacked, consist of the in-plane fiber, adopt needling process to introduce vertical fibers at thickness direction, making density is 0.50g/cm
3, thickness is the pseudo-three-dimensional preform of 220mm;
(2) at normal temperatures Resins, epoxy, thinner and solidifying agent are mixed and made into epoxy resin adhesive liquid by 100: 10: 20 mass ratio; Described thinner is butylglycidyl ether, and described solidifying agent is quadrol;
(3) epoxy resin adhesive liquid being sprayed at pseudo-three-dimensional preform surface formation thickness is the coating of 5mm, the pseudo-three-dimensional preform that then will form after the coating places in the curing oven, be to solidify 8h under 40 ℃ the condition in temperature, make pseudo-three-dimensional preform surface hardening typing;
(4) pseudo-three-dimensional preform after solidifying is placed impregnating autoclave, adopting viscosity is 500mPas, solids content be 60% ammonia resol as soaker, flood 12h vacuumizing under the condition;
(5) pseudo-three-dimensional preform behind dipping being placed charring furnace, is to carry out charing under 1200 ℃ the vacuum condition to process in temperature, when the density of pseudo-three-dimensional preform reaches 0.90g/cm
3In time, stops charing and processes, and furnace cooling obtains precast body;
(6) precast body is carried out mechanical workout, then the precast body after the mechanical workout is placed chemical vapor deposition stove, adopt Sweet natural gas as presoma, be to carry out the CVD coating under 1100 ℃ the condition to process in temperature, forming thickness on the precast body surface is the coating of 150 μ m, it is 1800mm that furnace cooling namely obtains diameter, highly is 1500mm, and thickness is the polysilicon hydrogenation furnace carbon/carbon thermal insulation cover of 220mm.
The polysilicon hydrogenation furnace of the present embodiment preparation is 15MPa with the tensile strength of carbon/carbon thermal insulation cover, and compressive strength is 30MPa, and flexural strength is 25MPa, and thermal conductivity is 0.3W/mk (800 ℃).
Embodiment 4
The present embodiment is identical with embodiment 3 preparation methods, wherein difference is: described thinner is alcohol, acetone, toluene, epoxy propane butyl ether, propylene oxide phenyl ether or ethylene glycol diglycidylether, described solidifying agent is diethylenetriamine, triethylene tetramine or polymeric amide, adopts propylene as presoma.
The polysilicon hydrogenation furnace of the present embodiment preparation is 15MPa～25MPa with the tensile strength of carbon/carbon thermal insulation cover, compressive strength is 30MPa～50MPa, flexural strength is 25MPa～40MPa, and thermal conductivity is 0.3W/mk (800 ℃)～1.5W/mk (800 ℃).
Embodiment 5
(1) adopt charcoal cloth and short carbon fiber net tire alternative stacked, consist of the in-plane fiber, adopt needling process to introduce vertical fibers at thickness direction, making density is 0.35g/cm
3, thickness is the pseudo-three-dimensional preform of 160mm;
(2) at normal temperatures Resins, epoxy, thinner and solidifying agent are mixed and made into epoxy resin adhesive liquid by 100: 8: 14 mass ratio; Described thinner is epoxy propane butyl ether, and described solidifying agent is triethylene tetramine;
(3) epoxy resin adhesive liquid being brushed in pseudo-three-dimensional preform surface formation thickness is the coating of 2.8mm, the pseudo-three-dimensional preform that then will form after the coating places in the curing oven, be to solidify 2h under 80 ℃ the condition in temperature, make pseudo-three-dimensional preform surface hardening typing;
(4) pseudo-three-dimensional preform after solidifying is placed impregnating autoclave, adopting viscosity is 320mPas, solids content be 50% ammonia resol as soaker, flood 8h vacuumizing under the condition;
(5) pseudo-three-dimensional preform behind dipping being placed charring furnace, is to carry out charing under 1050 ℃ the vacuum condition to process in temperature, when the density of pseudo-three-dimensional preform reaches 0.75g/cm
3In time, stops charing and processes, and furnace cooling obtains precast body;
(6) precast body is carried out mechanical workout, then the precast body after the mechanical workout is placed chemical vapor deposition stove, adopt propylene as presoma, be to carry out the CVD coating under 950 ℃ the condition to process in temperature, forming thickness on the precast body surface is the coating of 75 μ m, it is 1400mm that furnace cooling namely obtains diameter, highly is 850mm, and thickness is the polysilicon hydrogenation furnace carbon/carbon thermal insulation cover of 150mm.
The polysilicon hydrogenation furnace of the present embodiment preparation is 25MPa with the tensile strength of carbon/carbon thermal insulation cover, and compressive strength is 50MPa, and flexural strength is 40MPa, and thermal conductivity is 1.5W/mk (800 ℃).
Embodiment 6
The present embodiment is identical with embodiment 5 preparation methods, wherein difference is: described thinner is alcohol, acetone, toluene, butylglycidyl ether, propylene oxide phenyl ether or ethylene glycol diglycidylether, described solidifying agent is diethylenetriamine, quadrol or polymeric amide, adopts Sweet natural gas as presoma.
The polysilicon hydrogenation furnace of the present embodiment preparation is 15MPa～25MPa with the tensile strength of carbon/carbon thermal insulation cover, compressive strength is 30MPa～50MPa, flexural strength is 25MPa～40MPa, and thermal conductivity is 0.3W/mk (800 ℃)～1.5W/mk (800 ℃).
Embodiment 7
(1) adopt charcoal cloth and short carbon fiber net tire alternative stacked, consist of the in-plane fiber, adopt needling process to introduce vertical fibers at thickness direction, making density is 0.50g/cm
3, thickness is the pseudo-three-dimensional preform of 100mm;
(2) at normal temperatures Resins, epoxy, thinner and solidifying agent are mixed and made into epoxy resin adhesive liquid by 100: 10: 8 mass ratio; Described thinner is the propylene oxide phenyl ether, and described solidifying agent is polymeric amide;
(3) epoxy resin adhesive liquid being sprayed at pseudo-three-dimensional preform surface formation thickness is the coating of 0.5mm, the pseudo-three-dimensional preform that then will form after the coating places in the curing oven, be to solidify 5h under 60 ℃ the condition in temperature, make pseudo-three-dimensional preform surface hardening typing;
(4) pseudo-three-dimensional preform after solidifying is placed impregnating autoclave, adopting viscosity is 300mPas, solids content be 40% ammonia resol as soaker, flood 12h vacuumizing under the condition;
(5) pseudo-three-dimensional preform behind dipping being placed charring furnace, is to carry out charing under 900 ℃ the vacuum condition to process in temperature, when the density of pseudo-three-dimensional preform reaches 0.80g/cm
3In time, stops charing and processes, and furnace cooling obtains precast body;
(6) precast body is carried out mechanical workout, then the precast body after the mechanical workout is placed chemical vapor deposition stove, adopt Sweet natural gas as presoma, be to carry out the CVD coating under 1000 ℃ the condition to process in temperature, forming thickness on the precast body surface is the coating of 100 μ m, it is 1500mm that furnace cooling namely obtains diameter, highly is 1000mm, and thickness is the polysilicon hydrogenation furnace carbon/carbon thermal insulation cover of 80mm.
The polysilicon hydrogenation furnace of the present embodiment preparation is 20MPa with the tensile strength of carbon/carbon thermal insulation cover, and compressive strength is 40MPa, and flexural strength is 30MPa, and thermal conductivity is 0.9W/mk (800 ℃).
Embodiment 8
The present embodiment is identical with embodiment 7 preparation methods, wherein difference is: described thinner is alcohol, acetone, toluene, butylglycidyl ether, epoxy propane butyl ether or ethylene glycol diglycidylether, described solidifying agent is diethylenetriamine, quadrol or triethylene tetramine, adopts propylene as presoma.
The polysilicon hydrogenation furnace of the present embodiment preparation is 15MPa～25MPa with the tensile strength of carbon/carbon thermal insulation cover, compressive strength is 30MPa～50MPa, flexural strength is 25MPa～40MPa, and thermal conductivity is 0.3W/mk (800 ℃)～1.5W/mk (800 ℃).
Claims (4)
1. the preparation method of a thick carbon/carbon heat insulation cover for polysilicon hydrogenation furnace is characterized in that, the method may further comprise the steps:
(1) adopt charcoal cloth and short carbon fiber to prepare pseudo-three-dimensional preform; The density of described pseudo-three-dimensional preform is 0.20g/cm
3～0.50g/cm
3, thickness is 100mm～220mm;
(2) at normal temperatures Resins, epoxy, thinner and solidifying agent are mixed and made into epoxy resin adhesive liquid by 100: 5～10: 8～20 mass ratio; Described thinner is alcohol, acetone, toluene or epoxide resin reactive diluent, and described solidifying agent is diethylenetriamine, quadrol, triethylene tetramine or polymeric amide;
(3) with epoxy resin adhesive liquid described in the step (2) spraying or brush that to form thickness in the surface of pseudo-three-dimensional preform described in the step (1) be the coating of 0.5mm～5mm, then will form pseudo-three-dimensional preform after the coating and solidify the pseudo-three-dimensional preform surface hardening is finalized the design;
(4) pseudo-three-dimensional preform after solidifying in the step (3) is placed impregnating autoclave, adopt ammonia resol as soaker, flood 4h～12h vacuumizing under the condition; The viscosity of described ammonia resol is 150mPas～500mPas, and the solids content of described ammonia resol is 40%～60%;
(5) pseudo-three-dimensional preform behind dipping in the step (4) is placed charring furnace, under the condition that vacuumizes, carry out charing and process, when the density of pseudo-three-dimensional preform reaches 0.60g/cm
3～0.90g/cm
3In time, stops charing and processes, and furnace cooling obtains precast body;
(6) precast body described in the step (5) is carried out mechanical workout, then the precast body after the mechanical workout being placed chemical vapor deposition stove to carry out the CVD coating processes, stopping the CVD coating after the precast body surface forms the coating that thickness is 5 μ m～150 μ m processes, it is 1000mm～1800mm that furnace cooling namely obtains diameter, highly be 200mm～1500mm, thickness is the polysilicon hydrogenation furnace carbon/carbon thermal insulation cover of 80mm～220mm; The system that described CVD coating is processed is: adopting propylene or Sweet natural gas as presoma, is to carry out the CVD coating under 800 ℃～1100 ℃ the condition to process in temperature.
2. the preparation method of a kind of thick carbon/carbon heat insulation cover for polysilicon hydrogenation furnace according to claim 1, it is characterized in that, epoxide resin reactive diluent described in the step (2) is butylglycidyl ether, epoxy propane butyl ether, propylene oxide phenyl ether or ethylene glycol diglycidylether.
3. the preparation method of a kind of thick carbon/carbon heat insulation cover for polysilicon hydrogenation furnace according to claim 1, it is characterized in that, the system of solidifying described in the step (3) is: place at normal temperatures 48h above solidify or place in the curing oven under temperature is 40 ℃～80 ℃ condition solidify 2h～8h.
4. the preparation method of a kind of thick carbon/carbon heat insulation cover for polysilicon hydrogenation furnace according to claim 1 is characterized in that, the temperature that charing described in the step (5) is processed is 900 ℃～1200 ℃.
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| CN102557037B (en) * | 2011-12-26 | 2013-06-19 | 湖南南方搏云新材料有限责任公司 | Heat-insulation corrosion-resistant structure of hydrogenation furnace |
| CN102990799B (en) * | 2012-08-17 | 2016-02-24 | 江苏天鸟高新技术股份有限公司 | The preparation method of polysilicon hydrogenation furnace thermal field band muscle insulation cover carbon fabric perform |
| CN103640319A (en) * | 2013-11-25 | 2014-03-19 | 宜兴市飞舟高新科技材料有限公司 | Making method for carbon fiber composite board preform |
| CN108046821A (en) * | 2018-01-24 | 2018-05-18 | 航天睿特碳材料有限公司 | A kind of preparation method of polycrystalline silicon ingot or purifying furnace carbon carbon lid plate |
| CN111960843A (en) * | 2020-08-31 | 2020-11-20 | 陕西美兰德炭素有限责任公司 | Method for shaping carbon fiber preform |
| CN112723898A (en) * | 2020-12-30 | 2021-04-30 | 内蒙古栢特新材料科技有限公司 | Preparation method of carbon/carbon liner for natural gas chemical vapor deposition furnace |
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| C06 | Publication | ||
| PB01 | Publication | ||
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